#------------------------------------------------------------------------------
#$Date: 2021-03-05 04:10:13 +0200 (Fri, 05 Mar 2021) $
#$Revision: 262662 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/57/7705777.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7705777
loop_
_publ_author_name
'Plajer, Alex J.'
'Crusius, Daniel'
'Jethwa, Rajesh B.'
'García-Romero, Álvaro'
'Bond, Andrew D.'
'García-Rodríguez, Raúl'
'Wright, Dominic S.'
_publ_section_title
;
 Coordination chemistry of the bench-stable tris-2-pyridyl pnictogen
 ligands [E(6-Me-2-py)₃] (E = As, As[double bond, length as
 m-dash]O, Sb).
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2393
_journal_page_last               2402
_journal_paper_doi               10.1039/d0dt03732j
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C18 H18 As Br2 N3 Ni'
_chemical_formula_sum            'C18 H18 As Br2 N3 Ni'
_chemical_formula_weight         569.80
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2020-10-20 deposited with the CCDC.	2020-11-26 downloaded from the CCDC.
;
_cell_angle_alpha                100.351(2)
_cell_angle_beta                 93.784(2)
_cell_angle_gamma                114.9694(15)
_cell_formula_units_Z            2
_cell_length_a                   8.2096(3)
_cell_length_b                   8.5804(3)
_cell_length_c                   15.8305(5)
_cell_measurement_reflns_used    4761
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      66.55
_cell_measurement_theta_min      2.87
_cell_volume                     981.79(6)
_computing_cell_refinement       'SAINT (Bruker, 2016)'
_computing_data_collection       'APEX3 (Bruker, 2016)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  SHELXL
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker D8-QUEST PHOTON-100'
_diffrn_measurement_method       'ω and φ-scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0527
_diffrn_reflns_av_unetI/netI     0.0507
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11093
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        66.844
_diffrn_reflns_theta_max         66.844
_diffrn_reflns_theta_min         2.874
_diffrn_source                   'Incoatec I\mS Cu microsource'
_exptl_absorpt_coefficient_mu    8.107
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.5763
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.927
_exptl_crystal_description       plate
_exptl_crystal_F_000             556
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.443
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         3463
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0332
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0253P)²+0.1532P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0616
_refine_ls_wR_factor_ref         0.0681
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2687
_reflns_number_total             3463
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt03732j2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 7705770--7705782.cif.'
_cod_database_code               7705777
_cambridge_user_name             'Alex Plajer'
_cambridge_user_crsid            ajp233
_cambridge_supervisor_name       'Dominic Wright'
_cambridge_supervisor_crsid      dsw1000
_cambridge_crystallographer_name 'Andrew Bond'
_cambridge_crystallographer_crsid adb29
_cambridge_sample_id             DC_NiBr2As(III)
_cambridge_data_id               DW_B1_0288
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.419
_shelx_estimated_absorpt_t_max   0.923
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
As1 As 0.71657(6) 0.57982(6) 0.21365(3) 0.02103(12) Uani 1 1 d . . . . .
Br1 Br 0.03257(6) 0.19946(6) 0.08826(3) 0.02686(13) Uani 1 1 d . . . . .
Br2 Br 0.18352(7) 0.56454(7) 0.33775(3) 0.03538(14) Uani 1 1 d . . . . .
Ni1 Ni 0.24055(9) 0.42189(9) 0.21020(4) 0.01887(17) Uani 1 1 d . . . . .
N1 N 0.7206(5) 0.8545(5) 0.3425(2) 0.0269(8) Uani 1 1 d . . . . .
N2 N 0.3835(4) 0.2874(4) 0.2337(2) 0.0208(8) Uani 1 1 d . . . . .
N3 N 0.3872(4) 0.6017(4) 0.1448(2) 0.0165(7) Uani 1 1 d . . . . .
C1 C 0.6959(6) 0.6881(6) 0.3310(3) 0.0244(10) Uani 1 1 d . . . . .
C2 C 0.6855(7) 0.6032(7) 0.3977(3) 0.0439(14) Uani 1 1 d . . . . .
H2A H 0.671959 0.485517 0.387061 0.053 Uiso 1 1 calc R U . . .
C3 C 0.6952(8) 0.6946(8) 0.4806(3) 0.0578(18) Uani 1 1 d . . . . .
H3A H 0.686765 0.639721 0.528293 0.069 Uiso 1 1 calc R U . . .
C4 C 0.7169(8) 0.8617(9) 0.4933(3) 0.0569(17) Uani 1 1 d . . . . .
H4A H 0.721885 0.924801 0.550018 0.068 Uiso 1 1 calc R U . . .
C5 C 0.7319(7) 0.9422(7) 0.4238(3) 0.0373(12) Uani 1 1 d . . . . .
C6 C 0.7676(9) 1.1346(8) 0.4361(4) 0.0615(18) Uani 1 1 d . . . . .
H6A H 0.822712 1.180846 0.387422 0.092 Uiso 1 1 calc R U . . .
H6B H 0.850581 1.203844 0.490704 0.092 Uiso 1 1 calc R U . . .
H6C H 0.652417 1.142987 0.438071 0.092 Uiso 1 1 calc R U . . .
C7 C 0.5566(6) 0.3372(5) 0.2168(3) 0.0212(9) Uani 1 1 d . . . . .
C8 C 0.6396(7) 0.2265(6) 0.2137(3) 0.0304(11) Uani 1 1 d . . . . .
H8A H 0.757587 0.261528 0.198023 0.036 Uiso 1 1 calc R U . . .
C9 C 0.5489(7) 0.0636(6) 0.2337(3) 0.0379(12) Uani 1 1 d . . . . .
H9A H 0.602476 -0.015722 0.231135 0.046 Uiso 1 1 calc R U . . .
C10 C 0.3809(7) 0.0197(6) 0.2571(3) 0.0344(12) Uani 1 1 d . . . . .
H10A H 0.320027 -0.088256 0.274465 0.041 Uiso 1 1 calc R U . . .
C11 C 0.2984(6) 0.1298(6) 0.2559(3) 0.0252(10) Uani 1 1 d . . . . .
C12 C 0.1092(6) 0.0765(6) 0.2779(3) 0.0387(13) Uani 1 1 d . . . . .
H12A H 0.100572 0.180603 0.310283 0.058 Uiso 1 1 calc R U . . .
H12B H 0.083301 -0.011055 0.313481 0.058 Uiso 1 1 calc R U . . .
H12C H 0.020655 0.025145 0.224072 0.058 Uiso 1 1 calc R U . . .
C13 C 0.5640(5) 0.6411(5) 0.1390(2) 0.0177(9) Uani 1 1 d . . . . .
C14 C 0.6528(6) 0.7323(6) 0.0794(3) 0.0235(10) Uani 1 1 d . . . . .
H14A H 0.776229 0.757298 0.076198 0.028 Uiso 1 1 calc R U . . .
C15 C 0.5605(6) 0.7869(6) 0.0246(3) 0.0257(10) Uani 1 1 d . . . . .
H15A H 0.617739 0.845780 -0.018321 0.031 Uiso 1 1 calc R U . . .
C16 C 0.3835(6) 0.7543(6) 0.0332(3) 0.0250(10) Uani 1 1 d . . . . .
H16A H 0.318227 0.792537 -0.003156 0.030 Uiso 1 1 calc R U . . .
C17 C 0.3016(5) 0.6657(5) 0.0950(2) 0.0199(9) Uani 1 1 d . . . . .
C18 C 0.1126(5) 0.6382(6) 0.1080(3) 0.0256(10) Uani 1 1 d . . . . .
H18A H 0.104460 0.652726 0.170181 0.038 Uiso 1 1 calc R U . . .
H18B H 0.024907 0.518838 0.076784 0.038 Uiso 1 1 calc R U . . .
H18C H 0.085168 0.725148 0.085536 0.038 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As -0.9300 1.0051 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C7 As1 C13 103.09(17) . . ?
C7 As1 C1 96.02(17) . . ?
C13 As1 C1 102.01(17) . . ?
N3 Ni1 N2 107.07(13) . . ?
N3 Ni1 Br2 109.83(9) . . ?
N2 Ni1 Br2 112.97(10) . . ?
N3 Ni1 Br1 98.34(9) . . ?
N2 Ni1 Br1 95.76(10) . . ?
Br2 Ni1 Br1 130.23(3) . . ?
C1 N1 C5 117.8(4) . . ?
C11 N2 C7 117.9(4) . . ?
C11 N2 Ni1 119.5(3) . . ?
C7 N2 Ni1 122.0(3) . . ?
C17 N3 C13 118.3(3) . . ?
C17 N3 Ni1 119.2(3) . . ?
C13 N3 Ni1 121.8(3) . . ?
N1 C1 C2 123.6(4) . . ?
N1 C1 As1 115.3(3) . . ?
C2 C1 As1 120.3(4) . . ?
C1 C2 C3 117.8(5) . . ?
C1 C2 H2A 121.1 . . ?
C3 C2 H2A 121.1 . . ?
C4 C3 C2 119.4(5) . . ?
C4 C3 H3A 120.3 . . ?
C2 C3 H3A 120.3 . . ?
C3 C4 C5 120.2(5) . . ?
C3 C4 H4A 119.9 . . ?
C5 C4 H4A 119.9 . . ?
N1 C5 C4 121.2(5) . . ?
N1 C5 C6 116.9(4) . . ?
C4 C5 C6 121.9(5) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N2 C7 C8 122.1(4) . . ?
N2 C7 As1 122.3(3) . . ?
C8 C7 As1 115.0(3) . . ?
C7 C8 C9 119.2(4) . . ?
C7 C8 H8A 120.4 . . ?
C9 C8 H8A 120.4 . . ?
C10 C9 C8 118.4(4) . . ?
C10 C9 H9A 120.8 . . ?
C8 C9 H9A 120.8 . . ?
C9 C10 C11 120.9(4) . . ?
C9 C10 H10A 119.5 . . ?
C11 C10 H10A 119.5 . . ?
N2 C11 C10 121.1(4) . . ?
N2 C11 C12 118.3(4) . . ?
C10 C11 C12 120.6(4) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N3 C13 C14 121.9(4) . . ?
N3 C13 As1 124.1(3) . . ?
C14 C13 As1 114.0(3) . . ?
C15 C14 C13 119.3(4) . . ?
C15 C14 H14A 120.3 . . ?
C13 C14 H14A 120.3 . . ?
C14 C15 C16 118.8(4) . . ?
C14 C15 H15A 120.6 . . ?
C16 C15 H15A 120.6 . . ?
C15 C16 C17 119.7(4) . . ?
C15 C16 H16A 120.1 . . ?
C17 C16 H16A 120.1 . . ?
N3 C17 C16 121.7(4) . . ?
N3 C17 C18 118.3(3) . . ?
C16 C17 C18 120.0(4) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
As1 C7 1.949(4) . ?
As1 C13 1.957(4) . ?
As1 C1 1.975(4) . ?
Br1 Ni1 2.4029(8) . ?
Br2 Ni1 2.3484(8) . ?
Ni1 N3 2.018(3) . ?
Ni1 N2 2.022(4) . ?
N1 C1 1.330(6) . ?
N1 C5 1.345(6) . ?
N2 C11 1.358(5) . ?
N2 C7 1.360(5) . ?
N3 C17 1.351(5) . ?
N3 C13 1.358(5) . ?
C1 C2 1.373(6) . ?
C2 C3 1.382(7) . ?
C2 H2A 0.9500 . ?
C3 C4 1.343(9) . ?
C3 H3A 0.9500 . ?
C4 C5 1.386(7) . ?
C4 H4A 0.9500 . ?
C5 C6 1.522(8) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C8 1.380(6) . ?
C8 C9 1.386(7) . ?
C8 H8A 0.9500 . ?
C9 C10 1.364(7) . ?
C9 H9A 0.9500 . ?
C10 C11 1.377(6) . ?
C10 H10A 0.9500 . ?
C11 C12 1.507(6) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.381(5) . ?
C14 C15 1.380(6) . ?
C14 H14A 0.9500 . ?
C15 C16 1.380(6) . ?
C15 H15A 0.9500 . ?
C16 C17 1.381(5) . ?
C16 H16A 0.9500 . ?
C17 C18 1.502(6) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 N1 C1 C2 -1.5(7) . . . . ?
C5 N1 C1 As1 -171.4(3) . . . . ?
N1 C1 C2 C3 2.2(8) . . . . ?
As1 C1 C2 C3 171.7(4) . . . . ?
C1 C2 C3 C4 -0.9(9) . . . . ?
C2 C3 C4 C5 -0.9(10) . . . . ?
C1 N1 C5 C4 -0.5(7) . . . . ?
C1 N1 C5 C6 177.7(5) . . . . ?
C3 C4 C5 N1 1.7(9) . . . . ?
C3 C4 C5 C6 -176.4(6) . . . . ?
C11 N2 C7 C8 6.1(6) . . . . ?
Ni1 N2 C7 C8 -164.9(3) . . . . ?
C11 N2 C7 As1 -163.9(3) . . . . ?
Ni1 N2 C7 As1 25.0(4) . . . . ?
N2 C7 C8 C9 -4.1(7) . . . . ?
As1 C7 C8 C9 166.6(3) . . . . ?
C7 C8 C9 C10 -1.0(7) . . . . ?
C8 C9 C10 C11 3.9(7) . . . . ?
C7 N2 C11 C10 -3.1(6) . . . . ?
Ni1 N2 C11 C10 168.2(3) . . . . ?
C7 N2 C11 C12 177.9(4) . . . . ?
Ni1 N2 C11 C12 -10.8(5) . . . . ?
C9 C10 C11 N2 -1.8(7) . . . . ?
C9 C10 C11 C12 177.1(4) . . . . ?
C17 N3 C13 C14 -5.0(6) . . . . ?
Ni1 N3 C13 C14 165.2(3) . . . . ?
C17 N3 C13 As1 173.9(3) . . . . ?
Ni1 N3 C13 As1 -15.9(4) . . . . ?
N3 C13 C14 C15 0.7(6) . . . . ?
As1 C13 C14 C15 -178.3(3) . . . . ?
C13 C14 C15 C16 2.4(6) . . . . ?
C14 C15 C16 C17 -1.1(7) . . . . ?
C13 N3 C17 C16 6.4(6) . . . . ?
Ni1 N3 C17 C16 -164.1(3) . . . . ?
C13 N3 C17 C18 -173.8(4) . . . . ?
Ni1 N3 C17 C18 15.7(5) . . . . ?
C15 C16 C17 N3 -3.4(6) . . . . ?
C15 C16 C17 C18 176.8(4) . . . . ?
